US10683326B2ActiveUtilityA1

Crystalline salt forms

93
Assignee: STEALTH BIOTHERAPEUTICS CORPPriority: Mar 11, 2016Filed: Mar 10, 2017Granted: Jun 16, 2020
Est. expiryMar 11, 2036(~9.7 yrs left)· nominal 20-yr term from priority
C07K 5/1005C07J 31/006C07C 309/30C07C 309/04C07C 63/08C07C 57/15C07C 55/07C07B 2200/13C07B 2200/07A61P 39/06C07C 55/10A61K 38/00A61P 43/00C07K 5/1019A61P 27/02C07K 5/0817
93
PatentIndex Score
6
Cited by
13
References
15
Claims

Abstract

Disclosed are various crystalline salt forms of D-Arg-Dmt-Lys-Phe-NH2.

Claims

exact text as granted — not AI-modified
What is claimed is: 
     
       1. A crystalline form of a salt of Compound I, 
       
         
           
           
               
               
           
         
         wherein said crystalline form has peaks in its XRPD pattern at values of two theta as listed in any one of Tables 1′-20′; 
         wherein Table 1′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                    4.9500 
                 
                    5.7914 
                 
                    8.5140 
                 
                    9.8145 
                 
                   10.5199 
                 
                   11.9028 
                 
                   12.3400 
                 
                   12.6450 
                 
                   13.1574 
                 
                   16.0665 
                 
                   16.7594 
                 
                   17.0428 
                 
                   19.0804 
                 
                   20.3368 
                 
                   20.7068 
                 
                   21.7397 
                 
                     
                 
             
                
                
                
               
               
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 2′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                    7.4205 
                 
                    9.8832 
                 
                   12.4010 
                 
                   13.0698 
                 
                   13.3833 
                 
                   14.4079 
                 
                   15.0973 
                 
                   15.5537 
                 
                   16.2771 
                 
                   16.8114 
                 
                   17.1732 
                 
                   17.4697 
                 
                   17.7008 
                 
                   19.4681 
                 
                   19.8491 
                 
                   22.8297 
                 
                   29.9651 
                 
                   32.5913 
                 
                     
                 
             
                
                
                
               
               
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 3′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                    6.3236 
                 
                    7.1904 
                 
                    9.0662 
                 
                   11.1993 
                 
                   11.6515 
                 
                   11.8245 
                 
                   12.2481 
                 
                   12.7291 
                 
                   12.9196 
                 
                   13.4259 
                 
                   13.9356 
                 
                   14.0866 
                 
                   14.3102 
                 
                   14.7230 
                 
                   15.3518 
                 
                   15.7767 
                 
                   16.0824 
                 
                   16.6610 
                 
                   16.9655 
                 
                   17.4222 
                 
                   18.1176 
                 
                   18.9399 
                 
                   19.5396 
                 
                   19.7829 
                 
                   34.7854 
                 
                   20.0556 
                 
                   20.2220 
                 
                   21.6820 
                 
                   22.4522 
                 
                   22.7058 
                 
                   23.1326 
                 
                   23.3451 
                 
                   23.7455 
                 
                   24.2204 
                 
                   24.5976 
                 
                   24.7839 
                 
                   25.6635 
                 
                   25.9383 
                 
                   27.0486 
                 
                   27.7138 
                 
                   28.2876 
                 
                   28.5866 
                 
                   28.8350 
                 
                   29.4111 
                 
                   29.7366 
                 
                   30.9351 
                 
                   31.2970 
                 
                   31.8586 
                 
                   34.1666 
                 
                     
                 
             
                
                
                
               
               
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 4′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                    6.5048 
                 
                    7.0412 
                 
                    9.0165 
                 
                   11.5522 
                 
                   11.8465 
                 
                   12.0031 
                 
                   12.4973 
                 
                   13.0115 
                 
                   13.2622 
                 
                   14.2951 
                 
                   14.4394 
                 
                   14.6700 
                 
                   15.0149 
                 
                   15.7182 
                 
                   15.8732 
                 
                   16.0677 
                 
                   17.3224 
                 
                   17.6596 
                 
                   18.0742 
                 
                   19.3625 
                 
                   19.5565 
                 
                   19.6954 
                 
                   20.0052 
                 
                   20.5458 
                 
                   21.1722 
                 
                   21.9749 
                 
                   22.4132 
                 
                   22.7633 
                 
                   23.1157 
                 
                   23.4474 
                 
                   23.7123 
                 
                   24.2578 
                 
                   24.5249 
                 
                   25.0281 
                 
                   25.2220 
                 
                   25.4124 
                 
                   26.1017 
                 
                   26.4002 
                 
                   26.6640 
                 
                   27.2584 
                 
                   27.6862 
                 
                   28.2087 
                 
                   28.4358 
                 
                   28.6690 
                 
                   29.0632 
                 
                   29.7900 
                 
                   30.1856 
                 
                   31.7342 
                 
                   32.5306 
                 
                   34.2641 
                 
                     
                 
             
                
                
                
               
               
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 5′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                    5.6855 
                 
                    6.0206 
                 
                   10.3924 
                 
                   10.9552 
                 
                   11.1560 
                 
                   11.6500 
                 
                   12.0524 
                 
                   13.5772 
                 
                   13.8529 
                 
                   14.7106 
                 
                   14.9409 
                 
                   15.2690 
                 
                   15.7091 
                 
                   15.9920 
                 
                   17.0746 
                 
                   17.5076 
                 
                   17.9935 
                 
                   18.2959 
                 
                   18.5258 
                 
                   18.7728 
                 
                   19.6638 
                 
                   20.4019 
                 
                   20.8566 
                 
                   21.2027 
                 
                   21.3736 
                 
                   21.6173 
                 
                   22.0030 
                 
                   22.1468 
                 
                   22.4678 
                 
                   22.9236 
                 
                   23.4098 
                 
                   24.1636 
                 
                   24.6355 
                 
                   24.8676 
                 
                   25.2453 
                 
                   25.4632 
                 
                   25.9375 
                 
                   26.4465 
                 
                   27.2385 
                 
                   27.8576 
                 
                   28.1594 
                 
                   28.6842 
                 
                   29.1886 
                 
                   30.2331 
                 
                   30.8093 
                 
                   32.2440 
                 
                   32.6305 
                 
                   33.2034 
                 
                   33.6754 
                 
                   34.5344 
                 
                     
                 
             
                
                
                
               
               
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 6′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   3.2104 
                 
                   4.3126 
                 
                   5.9916 
                 
                   7.4447 
                 
                   9.3645 
                 
                   9.6885 
                 
                   9.9966 
                 
                   10.3209 
                 
                   11.8020 
                 
                   12.0313 
                 
                   12.3878 
                 
                   12.7870 
                 
                   13.6046 
                 
                   14.3857 
                 
                   14.5904 
                 
                   14.9160 
                 
                   15.1627 
                 
                   15.7759 
                 
                   15.9359 
                 
                   16.3636 
                 
                   17.5056 
                 
                   18.0062 
                 
                   18.4116 
                 
                   18.9363 
                 
                   19.4525 
                 
                   19.7728 
                 
                   20.1145 
                 
                   20.6143 
                 
                   21.3512 
                 
                   22.1408 
                 
                   22.7308 
                 
                   23.2392 
                 
                   23.8175 
                 
                   24.0397 
                 
                   24.8469 
                 
                   25.4521 
                 
                   26.0833 
                 
                   26.6795 
                 
                   27.1575 
                 
                   27.8454 
                 
                   28.7187 
                 
                   29.7607 
                 
                   31.1650 
                 
                   32.1555 
                 
                   33.2176 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 7′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   4.9532 
                 
                   6.1637 
                 
                   7.2943 
                 
                   7.7207 
                 
                   8.3148 
                 
                   9.8933 
                 
                   10.0378 
                 
                   12.2572 
                 
                   13.1795 
                 
                   13.3769 
                 
                   13.9612 
                 
                   14.5695 
                 
                   14.8668 
                 
                   15.0420 
                 
                   16.1696 
                 
                   16.4614 
                 
                   17.2938 
                 
                   18.0668 
                 
                   18.6224 
                 
                   19.4090 
                 
                   19.6513 
                 
                   20.1142 
                 
                   20.4050 
                 
                   20.6432 
                 
                   21.3207 
                 
                   22.0879 
                 
                   22.5352 
                 
                   22.8692 
                 
                   23.3140 
                 
                   24.0468 
                 
                   24.3692 
                 
                   24.7043 
                 
                   25.7054 
                 
                   26.1300 
                 
                   26.6847 
                 
                   27.4517 
                 
                   28.5093 
                 
                   29.3658 
                 
                   29.8396 
                 
                   30.2682 
                 
                   31.3451 
                 
                   31.6554 
                 
                   33.2878 
                 
                   34.2219 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 8′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   3.8204 
                 
                   4.2694 
                 
                   5.6244 
                 
                   6.5112 
                 
                   6.9639 
                 
                   8.1270 
                 
                   9.0666 
                 
                   10.3663 
                 
                   10.7413 
                 
                   11.3178 
                 
                   11.7667 
                 
                   12.3780 
                 
                   13.0244 
                 
                   13.6355 
                 
                   14.4623 
                 
                   14.8263 
                 
                   15.3745 
                 
                   15.7939 
                 
                   16.4008 
                 
                   16.9166 
                 
                   17.3729 
                 
                   17.6682 
                 
                   18.1633 
                 
                   18.3587 
                 
                   19.0634 
                 
                   19.8595 
                 
                   20.3863 
                 
                   20.7089 
                 
                   21.1449 
                 
                   22.3294 
                 
                   22.7660 
                 
                   23.1962 
                 
                   23.5383 
                 
                   23.9992 
                 
                   24.5505 
                 
                   24.9379 
                 
                   25.6244 
                 
                   26.9282 
                 
                   28.5609 
                 
                   29.4356 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 9′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   5.4182 
                 
                   5.7226 
                 
                   9.4519 
                 
                   9.7709 
                 
                   10.8340 
                 
                   11.0000 
                 
                   11.7890 
                 
                   13.3227 
                 
                   13.5503 
                 
                   13.9236 
                 
                   14.3536 
                 
                   14.6610 
                 
                   14.7960 
                 
                   15.0602 
                 
                   15.5639 
                 
                   15.7577 
                 
                   16.2767 
                 
                   17.1600 
                 
                   17.4509 
                 
                   17.6937 
                 
                   18.1813 
                 
                   18.8180 
                 
                   18.9824 
                 
                   19.6693 
                 
                   20.5851 
                 
                   21.0850 
                 
                   21.4834 
                 
                   21.7565 
                 
                   22.0457 
                 
                   22.3107 
                 
                   23.1703 
                 
                   23.7448 
                 
                   23.9081 
                 
                   24.4576 
                 
                   24.9599 
                 
                   25.5780 
                 
                   25.9086 
                 
                   26.6417 
                 
                   27.2891 
                 
                   27.5817 
                 
                   28.5785 
                 
                   28.9965 
                 
                   29.5971 
                 
                   30.1716 
                 
                   30.3897 
                 
                   31.0846 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 10′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   5.4123 
                 
                   9.6642 
                 
                   9.9532 
                 
                   10.7777 
                 
                   10.9908 
                 
                   11.8302 
                 
                   13.3865 
                 
                   13.9832 
                 
                   14.5130 
                 
                   15.0235 
                 
                   15.6073 
                 
                   15.9886 
                 
                   17.2884 
                 
                   17.7412 
                 
                   18.7012 
                 
                   19.5647 
                 
                   20.0217 
                 
                   21.0255 
                 
                   21.3918 
                 
                   22.0785 
                 
                   22.8159 
                 
                   23.6802 
                 
                   24.0516 
                 
                   25.8493 
                 
                   26.9534 
                 
                   27.7402 
                 
                   28.1612 
                 
                   29.2755 
                 
                   30.5014 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 11′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   3.6528 
                 
                   5.3346 
                 
                   6.1921 
                 
                   7.1693 
                 
                   7.2584 
                 
                   7.9555 
                 
                   8.2989 
                 
                   9.2514 
                 
                   10.5913 
                 
                   11.1450 
                 
                   12.0332 
                 
                   12.7127 
                 
                   13.1965 
                 
                   13.5693 
                 
                   13.8163 
                 
                   14.3773 
                 
                   14.6066 
                 
                   15.3422 
                 
                   15.5476 
                 
                   15.9810 
                 
                   16.6013 
                 
                   17.5327 
                 
                   17.8949 
                 
                   18.2706 
                 
                   19.0516 
                 
                   19.3988 
                 
                   19.8836 
                 
                   20.2075 
                 
                   20.3963 
                 
                   20.7842 
                 
                   21.1854 
                 
                   21.8139 
                 
                   22.0119 
                 
                   22.4021 
                 
                   22.6620 
                 
                   22.9995 
                 
                   23.2815 
                 
                   23.5370 
                 
                   23.9934 
                 
                   24.6748 
                 
                   24.8788 
                 
                   25.7236 
                 
                   26.0766 
                 
                   26.8205 
                 
                   27.8212 
                 
                   28.5683 
                 
                   28.9477 
                 
                   29.3638 
                 
                   30.7259 
                 
                   32.1373 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 12′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   4.2283 
                 
                   5.2902 
                 
                   5.7064 
                 
                   7.0087 
                 
                   7.2740 
                 
                   8.4471 
                 
                   10.2953 
                 
                   10.4698 
                 
                   11.1043 
                 
                   11.2764 
                 
                   11.6690 
                 
                   12.0243 
                 
                   12.3661 
                 
                   12.6972 
                 
                   13.0211 
                 
                   13.2807 
                 
                   14.8277 
                 
                   15.4615 
                 
                   15.8235 
                 
                   16.0773 
                 
                   16.9930 
                 
                   17.2436 
                 
                   18.1053 
                 
                   19.5434 
                 
                   20.7010 
                 
                   21.1934 
                 
                   21.9721 
                 
                   22.2605 
                 
                   22.6296 
                 
                   23.6035 
                 
                   23.7351 
                 
                   24.0613 
                 
                   24.4738 
                 
                   24.9772 
                 
                   25.5868 
                 
                   26.0270 
                 
                   27.2637 
                 
                   27.9596 
                 
                   28.5769 
                 
                   30.7356 
                 
                   31.2491 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 13′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   4.6078 
                 
                   4.7247 
                 
                   5.6369 
                 
                   5.7945 
                 
                   6.9083 
                 
                   7.2036 
                 
                   7.4378 
                 
                   9.2520 
                 
                   9.3801 
                 
                   10.0352 
                 
                   10.3048 
                 
                   11.1685 
                 
                   11.4467 
                 
                   11.7464 
                 
                   12.7059 
                 
                   13.1603 
                 
                   13.3277 
                 
                   13.6611 
                 
                   14.2278 
                 
                   14.6322 
                 
                   14.9188 
                 
                   15.0644 
                 
                   15.7469 
                 
                   15.9535 
                 
                   16.2032 
                 
                   16.3240 
                 
                   16.6769 
                 
                   17.4243 
                 
                   18.2889 
                 
                   18.8043 
                 
                   19.2960 
                 
                   19.5746 
                 
                   19.9329 
                 
                   20.2723 
                 
                   20.5228 
                 
                   21.1443 
                 
                   21.5244 
                 
                   21.7014 
                 
                   22.0764 
                 
                   22.3112 
                 
                   22.3752 
                 
                   22.6648 
                 
                   22.8586 
                 
                   23.1084 
                 
                   23.2825 
                 
                   23.5664 
                 
                   23.9441 
                 
                   24.1708 
                 
                   24.2438 
                 
                   24.5667 
                 
                   24.7979 
                 
                   25.2094 
                 
                   25.5564 
                 
                   26.3596 
                 
                   26.4901 
                 
                   26.8577 
                 
                   27.3567 
                 
                   27.6722 
                 
                   28.0031 
                 
                   28.3434 
                 
                   28.6121 
                 
                   29.0080 
                 
                   29.5671 
                 
                   30.6297 
                 
                   31.2974 
                 
                   31.9650 
                 
                   32.3013 
                 
                   33.4812 
                 
                   33.9277 
                 
                   34.2253 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 14′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   4.8468 
                 
                   7.2009 
                 
                   9.2287 
                 
                   9.8752 
                 
                   11.3790 
                 
                   12.3753 
                 
                   13.1003 
                 
                   13.3414 
                 
                   14.0505 
                 
                   14.4103 
                 
                   14.9682 
                 
                   15.5626 
                 
                   16.0210 
                 
                   16.2253 
                 
                   16.5208 
                 
                   16.8847 
                 
                   17.3260 
                 
                   18.0436 
                 
                   18.5063 
                 
                   19.5667 
                 
                   19.8049 
                 
                   20.4746 
                 
                   21.3412 
                 
                   21.6458 
                 
                   21.8878 
                 
                   22.4062 
                 
                   22.9397 
                 
                   23.2065 
                 
                   23.6258 
                 
                   23.8043 
                 
                   24.2839 
                 
                   24.5292 
                 
                   24.9422 
                 
                   25.6526 
                 
                   26.2095 
                 
                   26.5712 
                 
                   26.8039 
                 
                   27.3245 
                 
                   27.9402 
                 
                   28.3452 
                 
                   29.7807 
                 
                   30.4185 
                 
                   32.4348 
                 
                   33.9687 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 15′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   5.2173 
                 
                   6.5788 
                 
                   10.4657 
                 
                   11.9526 
                 
                   12.2981 
                 
                   12.9633 
                 
                   13.1469 
                 
                   13.6532 
                 
                   13.9226 
                 
                   14.0801 
                 
                   14.8387 
                 
                   15.2947 
                 
                   15.7415 
                 
                   16.0705 
                 
                   17.0800 
                 
                   17.8037 
                 
                   18.0998 
                 
                   19.2649 
                 
                   19.6536 
                 
                   20.4686 
                 
                   20.9891 
                 
                   21.5138 
                 
                   22.3786 
                 
                   23.1604 
                 
                   24.0181 
                 
                   24.7153 
                 
                   25.0063 
                 
                   25.3823 
                 
                   26.0374 
                 
                   26.3551 
                 
                   27.5053 
                 
                   28.0100 
                 
                   28.7269 
                 
                   31.3366 
                 
                   32.4594 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 16′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   6.6183 
                 
                   7.3884 
                 
                   7.6111 
                 
                   8.2981 
                 
                   8.8993 
                 
                   10.0751 
                 
                   11.1019 
                 
                   11.5582 
                 
                   11.8344 
                 
                   12.2224 
                 
                   12.9751 
                 
                   13.4040 
                 
                   13.8874 
                 
                   14.2668 
                 
                   14.4971 
                 
                   15.0582 
                 
                   15.7548 
                 
                   16.3188 
                 
                   17.3388 
                 
                   17.9628 
                 
                   18.5415 
                 
                   18.9064 
                 
                   19.4667 
                 
                   19.7556 
                 
                   20.1836 
                 
                   20.7747 
                 
                   21.5446 
                 
                   22.2369 
                 
                   22.6652 
                 
                   23.0991 
                 
                   23.6074 
                 
                   23.8948 
                 
                   24.1368 
                 
                   24.5986 
                 
                   25.2568 
                 
                   25.9952 
                 
                   26.9499 
                 
                   27.4845 
                 
                   27.8343 
                 
                   28.8828 
                 
                   29.2983 
                 
                   29.6677 
                 
                   30.1333 
                 
                   30.7281 
                 
                   31.5937 
                 
                   32.9662 
                 
                   33.8294 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 17′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   5.2074 
                 
                   6.5759 
                 
                   10.4268 
                 
                   11.9087 
                 
                   12.2972 
                 
                   12.8749 
                 
                   13.0948 
                 
                   13.6525 
                 
                   15.2610 
                 
                   15.7084 
                 
                   16.0248 
                 
                   16.4827 
                 
                   17.0200 
                 
                   17.7452 
                 
                   18.0663 
                 
                   19.2467 
                 
                   19.6260 
                 
                   20.4182 
                 
                   20.9504 
                 
                   21.1080 
                 
                   21.4534 
                 
                   22.2977 
                 
                   23.1512 
                 
                   23.9912 
                 
                   24.6413 
                 
                   24.9511 
                 
                   25.3280 
                 
                   25.9830 
                 
                   26.2805 
                 
                   27.4563 
                 
                   28.6746 
                 
                   29.6573 
                 
                   31.2290 
                 
                   32.3846 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 18′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   4.7133 
                 
                   7.0625 
                 
                   7.8327 
                 
                   9.4373 
                 
                   10.8320 
                 
                   11.2560 
                 
                   11.5530 
                 
                   12.1400 
                 
                   12.4180 
                 
                   13.2125 
                 
                   13.6676 
                 
                   14.1438 
                 
                   14.5314 
                 
                   14.8391 
                 
                   15.5031 
                 
                   15.6570 
                 
                   15.9242 
                 
                   16.2469 
                 
                   16.7975 
                 
                   18.0638 
                 
                   18.2986 
                 
                   18.6074 
                 
                   18.9236 
                 
                   19.0681 
                 
                   19.8194 
                 
                   20.2669 
                 
                   21.3752 
                 
                   21.6758 
                 
                   21.9446 
                 
                   22.6951 
                 
                   23.2295 
                 
                   23.6142 
                 
                   24.0109 
                 
                   24.4314 
                 
                   25.2281 
                 
                   25.5842 
                 
                   26.1514 
                 
                   26.7925 
                 
                   27.1916 
                 
                   28.1339 
                 
                   28.5109 
                 
                   29.2877 
                 
                   29.7222 
                 
                   30.6360 
                 
                   31.3505 
                 
                   32.6032 
                 
                   32.9347 
                 
                   33.8939 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         Table 19′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   5.0941 
                 
                   10.2223 
                 
                   11.8691 
                 
                   13.2023 
                 
                   13.7755 
                 
                   13.9773 
                 
                   14.6467 
                 
                   15.9075 
                 
                   16.7186 
                 
                   20.4020 
                 
                   21.9198 
                 
                   23.0969 
                 
                   23.5325 
                 
                   24.4800 
                 
                   25.2794 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
         and 
         Table 20′ is: 
       
       
         
           
                 
               
                     
                 
                   Pos. [°2θ] 
                 
                     
                 
                     
                 
                 
               
                   4.1731 
                 
                   5.1086 
                 
                   6.5676 
                 
                   7.9847 
                 
                   9.9321 
                 
                   10.3453 
                 
                   11.9442 
                 
                   13.1111 
                 
                   14.0979 
                 
                   14.5776 
                 
                   14.8894 
                 
                   15.4458 
                 
                   16.0064 
                 
                   17.5761 
                 
                   18.0178 
                 
                   18.5153 
                 
                   18.9551 
                 
                   19.2662 
                 
                   19.9186 
                 
                   20.3646 
                 
                   20.8102 
                 
                   21.1557 
                 
                   22.1676 
                 
                   22.3940 
                 
                   22.8184 
                 
                   23.2383 
                 
                   23.3762 
                 
                   24.1177 
                 
                   25.1899 
                 
                   25.5494 
                 
                   26.0776 
                 
                   27.5686 
                 
                     
                 
             
                
                
                
               
               
                
               
            
             
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
                
               
            
           
         
       
     
     
       2. A crystalline form of a salt of Compound I, 
       
         
           
           
               
               
           
         
         wherein said crystalline form has characteristic peaks in its XRPD pattern as described in any one of  FIGS. 1-26 . 
       
     
     
       3. The crystalline form of  claim 1 , wherein the crystalline form has peaks in its XRPD pattern at values of two theta as listed in any one of Tables 11′-18′. 
     
     
       4. The crystalline form of  claim 1 , wherein the crystalline form has peaks in its XRPD pattern at values of two theta as listed in any one of Tables 5′, 6′, 9′, and 10′. 
     
     
       5. The crystalline form of  claim 1 , wherein the crystalline form has peaks in its XRPD pattern at values of two theta as listed in any one of Tables 1′, 2′, 3′, 4′, 7′, 8′, 19′, and 20′. 
     
     
       6. A composition, comprising a crystalline form of  claim 1 . 
     
     
       7. A process for making a pharmaceutical composition comprising Compound I, 
       
         
           
           
               
               
           
         
         comprising dissolving a crystalline form of  claim 1 . 
       
     
     
       8. A composition, comprising a crystalline form of  claim 2 . 
     
     
       9. A composition, comprising a crystalline form of  claim 3 . 
     
     
       10. A composition, comprising a crystalline form of  claim 4 . 
     
     
       11. A composition, comprising a crystalline form of  claim 5 . 
     
     
       12. A process for making a pharmaceutical composition comprising Compound I, 
       
         
           
           
               
               
           
         
         comprising dissolving a crystalline form of  claim 2 . 
       
     
     
       13. A process for making a pharmaceutical composition comprising Compound I, 
       
         
           
           
               
               
           
         
         comprising dissolving a crystalline form of  claim 3 . 
       
     
     
       14. A process for making a pharmaceutical composition comprising Compound I, 
       
         
           
           
               
               
           
         
         comprising dissolving a crystalline form of  claim 4 . 
       
     
     
       15. A process for making a pharmaceutical composition comprising Compound I, 
       
         
           
           
               
               
           
         
         comprising dissolving a crystalline form of  claim 5 .

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